Process of separating beryllia from alumina and iron.



FRIEDRICH BEAN AND GABRIEL VAN ()ORDT, OF AIANNIIEIM, GERMANY.

PROCESS OF SEPARATING BEFIYLLIA FROM ALUMIN'A AND IRON- Specification of Letters Patent.

Patented May 21, 1907.

Application filed July 13, 1906. Serial No. 326,144.

To It when] it may 007113877'0:

Be it known that we, FRIEDRICH BRAN, residing at Mannheim, in the Grand Duchy of Baden. and Em ire of Germany, subject of the Emperor 0 Germany, and GABRIEL VAN OORDT, residing at Mannheim, in the Grand Duchy of Baden and Empire of Germany, subject of the Queen of the Netherlands, have invented certain new and useful Improvements in and Relating to a Process of Separating Beryllia from Alumina and Iron, of which the following: is a specification.

The object of the present case is to devise a simple, cheap and ready process of separating beryllia, sometimes called glucina, from alumina and also from iron oxid by treating a mixture. of the oxids with carbon dioxid, or bicarbonates', to dissolve beryllia while leaving alumina and iron oxid undissolvcd.

It is known that all forms of alumina precipitated from acid solutions if substantially pure hydra-ted alumina, are easily soluble in acids, even if weak or dilute, as for instance, acetic acid, while still fresh; that is, before they have been transformed into the so-called aged forms by time, heat or chemical agents. Similar precipitates of beryllia under like conditions pass more quickly into these aged forms; that is, into forms which are dillicultly' soluble in acids and alkalies.

()n this fact a separate method of separation is based.

As the result of experiment, it has been proved that un-aged forms of alumina and beryllia hydrates, that is forms still easily soluble in acids, respectively exhibit different behaviors toward acids and acid salts, particularly toward carbonic acid and its acid salts; thisdifi'erence de ending upon the dill'erent basicities and va encies of the hydroxids. The differences between these two hydrates in their reactions with, or solubilities in, acids and acid salts are still further accentuated if they have been obtained by decomposing their solutions in caustic alkali by means of carbon dioxid. 'Ihis differential behavior is es ecially marked as regards their reaction wit 1 carbonic acid or the bicarbonates, especially sodium bicarbonate.

When 'a mixture of alumina and beryllia hydrates, with some ferric hydrate, is precipitated from a caustic soda solution at 40 by carbon dioxid, or from a solution of the salts by heated alkali solution, all the beryllia and iron and considerable alumina are extracted from the precipitate by treatment with sulfuric acid of 10 B, with 1-0, per cent hydrochloric acid or with 10 per cent acetic acid, -while from the same precipitate tearbonic acid and bicarbonat dissolve only the beryllia with but traces iron and no alumina.

I-Ierzfeld and Korn (Ohem'ie der seltenen Erdcn, page 163) and C. Glaser (Chem'ische Zcimng, 189e, page 612) state that when salts of beryllia are precipitated by carbonate of sodium or bicarbc I only very dithcultlysoluble in carbonic acid in great excess, even when carbon dioxid is passed into the precipitation; Our experience is to the contrary. We have found that preci itated beryllium hydroxid and the so callmi .asic carbonates of beryllium are easily soluble in bicarbona'tes of alkali, with or without excess of carbon dio'xid, or in the carbonates if carbon d'i'oxid be passed into the liquid. The maximum of solubility is obtained when a molecule of the alkali M 0, is present for every molecule of beryllia. ()ther proportions may be used, but not so well, as involving either an unnecessary excess of alkali, or the possibility of some beryllia remaining undissolved.

While the statements from the cited an:

thorities would preclude the possibility of a separation of alumina from bervllia by any such reaction, (since the alleged behavior of ber 11m is practically that of alununa under $110 1 circumstances), as a matter of fact we ate, the precipitate is have found that. the diil'crence in behavior of the two is such as to allow a simple, cheap and ready process for their separation to be predicated u on it; a process resulting in a se aration wliich'is notv only technically usefu but quantitative. l or this separation, alkali is em )loyed, together with carbon dioxid, in such proportion as to obtain a carbonated compound wherein the alkali and beryllia are in the ratio of M. ,():BcO This carbonated compoundis soluble in water and is new-to chemistry. To obtain it, the beryllium hydroxid is treated either with an alkaline bicarbonate, such as sodium bicarbonate, in the correct proportion, or with an alkaline carbonate in solution, passing into the solution a stream of carbon dioxid. Carbon dioxid may be ate? In performing the separation of bcryllia treate from alumina, if the two hydroxids have been recipitated together they may be d with bicarbonate, with or without addition of carbon dioxid, or with-carbonate and carbon dioxid. The beryllia dissolves as the new compound. Or a saline solution of the two oxids may be treated with sufllcient alkali to neutralize the combined acid and also with enough more carbonated alkali and, if necessary, carbon dioxid, to furnish the stated compound with her llia. Berylha will remain in solution and a umnia precipitate. A solution of the two hydroxids in caustic alkali when treated with carbon throws down alumina. I As example of processes according to our invention may be adduced the following:

. 1. A mixture of hydroxids of iron, alumini-- um and beryllium, containing 4 parts of the iron oxid, parts alumina and 10 p arts beryllia, was treated with 100 arts by volume of a caustic soda solution. he solution was then filtered off undissolved ferric hydrate and treated with carbon and bicarbonate of treated with 62 or more parts of carbonate of sodium and enough water to make a double or triple normal solution. Into the mixture of carbonate solution and hydroxids, carbon dioxid was assed until all the carbonate was converte into bicarbonate, the resulting solution of the new beryllium compound separated from undissolved matters, as by filtration, and, the beryllia regained in solid fornrby heating, dilution or alkalization.

The same result was obtained by directly treating the same mixture of hydroxids with 88.6, or more, parts of sodium bicarbonate in saturated aqueous solution, either with or without passing more carbon dioxid into the solution. Filtration gave a solution of the new compound.-

With any of these methods, it the mixture of hydroxids was employed in excess, relative to the amount 1 alkali present, the solution filtered oi? from undissolved matters contains only the'new beryllium compound, a carbonated salt of alkali and berylha with the ratio of M 0 :BeO :1 :1 the symbolM designating either K or'Na.

The new compound is freely soluble in water and its'aqueous solution yields a precipitate upon heating, up omdilution, or upon addition otalkali or strong-acid.

What we claim is: 1-. The process ofse arating beryllia from alumina and iron whlc consists in treating a.

mixture containing thesame Withalkaliand carbon dioxid, said alkali being employed in amount sufficient to yield a carbonated com- I alumina and iron whic 1 consists in treating a mixture containing the same with a solution contammg'an alkali and carbon dioxid, sald alkali-being employed in amount sufliclent to yield a compound with the beryllia present wherein the ratio M' OzBeO subsists, and

4. The (process of forming a new beryllium I compoun which consists in treating beryllium hydroxidwith alkali and-carbon dioxid, said alkali being employed in amount suffi cient to form the ratio M OzBeO with theberyllia.

5. Thetprocess of forming a new beryllium compoun which consists in treating beryllium hydroxidwith dissolved alkali and car bon dioxid, said alkali being employed in amount sufficient to form the ratio M 0 :BeO

with the beryllia.

6; The (process of forming a new beryllium I .compoun amount that the contained alkali is sufficient In testimony whereof we hereunto affix our signatures in the presence of two witnesses.

FRIEDRIOH BRAN. GABRIEL VAN OORDT.

Witnesses 2 H. W. HARRIS,

Jos. H. LEUTE. I 

